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Lead-207 NMR Spectroscopy at 1.4 T: Application of Benchtop Instrumentation to a Challenging I = ½ Nucleus
Magnetic Resonance in Chemistry ( IF 2 ) Pub Date : 2020-07-16 , DOI: 10.1002/mrc.5036
Guy M Bernard 1 , Vladimir K Michaelis 1
Affiliation  

The practicality of obtaining liquid- and solid-state 207 Pb nuclear magnetic resonance (NMR) spectra with a low permanent-field magnet is investigated. Obtaining 207 Pb NMR spectra of salts in solution is shown to be viable for samples as dilute as 0.05 M. The concentration dependence of the 207 Pb chemical shifts for lead nitrate was investigated; the results are comparable to those obtained with high-field instruments. Likewise, the isotope effect of substituting D2 O for H2 O as the solvent was investigated and found to be comparable to those reported previously. Obtaining solid-state 207 Pb NMR spectra is challenging, but we demonstrate the ability to obtain such spectra for three unique solid samples. An axially symmetric 207 Pb powder pattern for lead nitrate and the powder pattern expected for lead chloride reveal linewidths dominated by shielding anisotropy, while 207 Pb-35/37 Cl J-coupling dominates in the methylammonium lead chloride perovskite material. Finally, recent innovations and the future potential of the instruments are considered.

中文翻译:

1.4 T 下的 Lead-207 NMR 光谱:台式仪器在具有挑战性的 I = ½ 核中的应用

研究了使用低永磁体获得液态和固态 207 Pb 核磁共振 (NMR) 谱的实用性。获得溶液中盐的 207 Pb NMR 谱表明对于稀释至 0.05 M 的样品是可行的。研究了硝酸铅的 207 Pb 化学位移的浓度依赖性;结果与使用高场仪器获得的结果相当。同样,研究了用 D2O 代替 H2O 作为溶剂的同位素效应,发现与之前报道的同位素效应相当。获得固态 207 Pb NMR 光谱具有挑战性,但我们证明了获得三种独特固体样品的此类光谱的能力。硝酸铅的轴对称 207 Pb 粉末图案和氯化铅的预期粉末图案显示线宽以屏蔽各向异性为主,而 207 Pb-35/37 Cl J 耦合在甲基氯化铵钙钛矿材料中占主导地位。最后,考虑了最近的创新和仪器的未来潜力。
更新日期:2020-07-16
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